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AOAC SPIFAN Nutrients ERP (April 26, 2017) Virtual Meeting Next Page
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AOAC SPIFAN Nutrients ERP (April 26, 2017) Virtual Meeting Next Page

 


AOAC SPIFAN Nutrients ERP (April 26, 2017) 		3
AOAC Policy Documents 		3
AOAC_Bylaws 		3
Antitrust 		15
Use of Association Name 		18
Volunteer Conflicts of Interest Policy 		115
Draft Meeting Agenda 		23
AOAC 2011.14-MTE 		25
TOC 		26
Collaborators 		27
Study Design 		28
Analytical Method 		28
Method Performance 		29
Safety Considerations 		109
Comments from Collaborators 		109
Conclusions 		110
Acknowledgements 		110
References 		110
AOAC 2016.03-Chloride 		111
AOAC 2016.03-Chloride MLT Final Report updated 		111
Summary 		111
STUDY DESCRIPTION 		114
Study Information 		114
Study Title 		114
Study Objective 		114
Study Directors 		114
Study Monitor 		114
Study Description 		114
Statistical evaluation 		115
Materials, Method and Laboratories 		115
Matrices 		115
Homogeneity Tests 		115
Method 		115
Participating laboratories 		115
Abbreviations 		116
Forms 		116
Cover Letters 		116
Sample Receipt Forms 		116
Reporting Templates 		116
INSTRUCTIONS TO PARTICIPANTS 		117
Part 1: Method set up and qualification of participants 		117
Practice Samples Receipt 		117
Analysis 		117
Timeline 		117
Reporting 		117
Laboratory Qualification 		117
Part 2: Multi-Laboratory Test Participation 		118
MLT Samples Receipt 		118
Analysis 		118
Timeline 		118
Reporting 		119
RESULTS 		119
Part 1. Method set up and qualification of participants 		119
Participation 		119
Method set up 		119
Practice samples results 		119
Part 2. Multi Laboratory Test 		119
Participation to MLT 		119
Results 		120
Conclusions 		121
Acknowledgments 		121
ANNEXES 		122
List of Annexes 		122
Annex A: List of Materials 		123
Practice Samples 		123
MLT Samples 		123
Annex B: Method 		124
1 Scope 		128
2 Principle 		128
3 Reagents 		129
3.1 Water, purified, greater than 18 MΩ (EMD Millipore1F ) Corp., Billerica, MA, USA, or equivalent). 		129
3.2 Sodium chloride (NaCl), purity ≥ 99,5 %), certified reference material for titrimetry, certified by BAM, according to ISO 17025—Sigma Aldrich #713871) or equivalent. 		129
3.3 Silver Nitrate (AgNO3), meets analytical specification of Ph. Eur., BP, USP, assay 99,8 % -100,5 %, Sigma-Aldrich 102201), or equivalent. 		129
3.4 Potassium ferrocyanide trihydrate (K4Fe(CN)6 3H2O), puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., ≥ 99%, Sigma-Aldrich # 315241) or equivalent. 		129
3.5 Zinc acetate dihydrate Zn(CH3COO)2 2H2O, ACS reagent puriss p.a., ≥ 99,0 %. Sigma Aldrich # 964591) or equivalent. 		129
3.6 Nitric acid (HNO3), minimum 65 % p.a., Merck #1004521), or equivalent. 		129
3.7 Standardized AgNO3 solution, 0,1 mol/l Titripur® Reag. Ph Eur,Reag. USP, # 1.09081.1000 or EM3214-1, or ready-to-use standardized titrant prepared according to GB/T 6011), or equivalent. 		129
3.8 Sodium chloride (NaCl) standardized solution, 0,100 mol/l +/- 0.5 % Alfa Aesar1), # 35616, (Ward Hill, MA, USA), or equivalent. 		129
3.9 Glacial acetic acid, 100 %, anhydrous for analysis EMSURE® ACS, ISO, Reag. Ph Eur MERCK, # 1000631) or equivalent. 		129
3.10 Potassium nitrate, (KNO3), for analysis EMSURE® ISO,Reag. Ph EurMERCK, # 1050631) or equivalent. 		129
3.11 Acetone, for cleaning of the electrode. Honeywell, # 010-4, (Muskegon, MI, USA) 1) or equivalent. 		129
3.12 Dimethylpolysiloxane, defoaming agent. Sigma-Aldrich, #DMPS2C1) or equivalent. 		129
4 Preparation of solutions 		129
4.1 Standardized AgNO3 solution, 0,1 mol/l. 		129
4.2 Sodium chloride solution, 0,1 mol/l. 		130
4.3 Precipitating solution (Carrez) I. 		130
4.4 Precipitating solution (Carrez) II. 		130
4.5 Nitric acid solution. 		130
4.6 Wash solution. 		130
4.7 AgNO3 solution, 0,025 mol/l (optional). 		130
4.8 NaCl solution, 0,025 mol/l (optional). 		130
4.9 KNO3 solution, 1 mol/l. 		130
5 Apparatus 		130
5.1 Analytical balance, precision 0,1 mg. 		131
5.2 Centrifuge, table-top with rotor for 50 ml conical tubes, capable of operating at ≥ 12 000 g. 		131
5.3 Centrifuge tubes, 50 ml, conical, polypropylene. 		131
5.4 Pipettes, 1 ml, 10 ml, 20 ml, 50 ml and 100 ml, Class A glass volumetric or automatic (Eppendorf or equivalent). 		131
5.5 One-mark volumetric flasks, 50 ml, 100 ml, 500 ml, and 1 000 ml glass, Class A. 		131
5.6 Autosampler Beaker, e.g. 120 ml, depending on the titrator used. 		131
5.7 pH-meter or mV-meter, with a scale covering ± 700 mV, and burette, 20 ml or 25 ml. 		131
5.8 Automatic titrator, (autosampler, motorized piston burette, with remote-control dispensing and filling). 		131
5.9 Combined ring silver electrode, e.g. Mettler DM 141 or DMi145-SC, Metrohm Ag Titrode 6.0430.100 or equivalent, alternatively a silver electrode with reference electrode. 		131
5.10 Magnetic stirrer, Heidolph MR 3000, or Metrohm 804Ti Stand with 802 Rod Stirrer, or equivalent. 		131
5.11 Water bath, Labotech DWM 16 or equivalent. 		131
5.12 Ultrasonic cleaner, Tianjin Auto Science AS2060B or equivalent. 		131
5.13 Disposable syringe, 3 ml, with handspike and 0,45 μm disposable syringe filter. 		131
6 Sample preparation 		131
7 Extraction 		131
7.1 General 		131
7.2 Weigh an appropriate aliquot of ready-to-feed (RTF) or reconstituted powder (e.g. 25 g) (accurate to 0,1 mg) into a 50 ml centrifuge tube. For samples with a high chloride content, weigh a smaller test portion e.g. 5 g of reconstituted or RTF prod... 		131
7.3 Transfer 2,5 ml precipitating solution I (4.3) and 2,5 ml precipitating solution II (4.4) into the tube. Complete to 50 ml with water. Mix well. If foam impacts the constant volume, one or two drops of defoaming agent (3.12) shall be used. 		132
7.4 Centrifuge at 12 000 g for 5 min at 4 C. Then equilibrate to room temperature. 		132
7.5 Accurately transfer either 10 ml supernatant from steps 7.2 to 7.4 or weigh an appropriate aliquot of RTF or reconstituted powder (e.g. 25 g accurate to 0,1 mg). For samples with a high chloride content, weigh a smaller test portion e.g. 5 g of re... 		132
7.6 The pH of the test solution shall be below 1,5. In case of any doubts, check by means of a pH-meter and, if necessary, add a little more nitric acid solution (4.5). 		132
8 Instrument operating conditions 		132
8.1 Check and maintenance of the combined silver electrode 		132
8.2 Titration 		132
8.3 Blank test: determination of reagent background content of chloride 		133
9 System suitability test 		133
10 Calculations 		133
11 Precision 		134
11.1 Repeatability 		134
11.2 Reproducibility 		134
12 Test report 		134
(informative) 		135
Annex D: Cover letters to participants 		139
Annex E: Receipt Forms 		140
Annex F: Reporting templates 		141
Annex G: Raw data MLT samples 		143
Cover letter: 		139
Samples Receipt Form 		140
AOAC 2016.03-Chloride All Samples/All Labs Results 		152-153
Summary of paired results 		152-153
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